CN1400073A - Pellet producing apparatus - Google Patents
Pellet producing apparatus Download PDFInfo
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- CN1400073A CN1400073A CN02127042A CN02127042A CN1400073A CN 1400073 A CN1400073 A CN 1400073A CN 02127042 A CN02127042 A CN 02127042A CN 02127042 A CN02127042 A CN 02127042A CN 1400073 A CN1400073 A CN 1400073A
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- ball
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- inclined plane
- cooling tower
- melted material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
- B01J2/02—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops
- B01J2/04—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops in a gaseous medium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
- B01J2/18—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic using a vibrating apparatus
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B07—SEPARATING SOLIDS FROM SOLIDS; SORTING
- B07B—SEPARATING SOLIDS FROM SOLIDS BY SIEVING, SCREENING, SIFTING OR BY USING GAS CURRENTS; SEPARATING BY OTHER DRY METHODS APPLICABLE TO BULK MATERIAL, e.g. LOOSE ARTICLES FIT TO BE HANDLED LIKE BULK MATERIAL
- B07B13/00—Grading or sorting solid materials by dry methods, not otherwise provided for; Sorting articles otherwise than by indirectly controlled devices
- B07B13/003—Separation of articles by differences in their geometrical form or by difference in their physical properties, e.g. elasticity, compressibility, hardness
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B07—SEPARATING SOLIDS FROM SOLIDS; SORTING
- B07B—SEPARATING SOLIDS FROM SOLIDS BY SIEVING, SCREENING, SIFTING OR BY USING GAS CURRENTS; SEPARATING BY OTHER DRY METHODS APPLICABLE TO BULK MATERIAL, e.g. LOOSE ARTICLES FIT TO BE HANDLED LIKE BULK MATERIAL
- B07B13/00—Grading or sorting solid materials by dry methods, not otherwise provided for; Sorting articles otherwise than by indirectly controlled devices
- B07B13/10—Grading or sorting solid materials by dry methods, not otherwise provided for; Sorting articles otherwise than by indirectly controlled devices using momentum effects
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B07—SEPARATING SOLIDS FROM SOLIDS; SORTING
- B07B—SEPARATING SOLIDS FROM SOLIDS BY SIEVING, SCREENING, SIFTING OR BY USING GAS CURRENTS; SEPARATING BY OTHER DRY METHODS APPLICABLE TO BULK MATERIAL, e.g. LOOSE ARTICLES FIT TO BE HANDLED LIKE BULK MATERIAL
- B07B13/00—Grading or sorting solid materials by dry methods, not otherwise provided for; Sorting articles otherwise than by indirectly controlled devices
- B07B13/10—Grading or sorting solid materials by dry methods, not otherwise provided for; Sorting articles otherwise than by indirectly controlled devices using momentum effects
- B07B13/11—Grading or sorting solid materials by dry methods, not otherwise provided for; Sorting articles otherwise than by indirectly controlled devices using momentum effects involving travel of particles over surfaces which separate by centrifugal force or by relative friction between particles and such surfaces, e.g. helical sorters
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B07—SEPARATING SOLIDS FROM SOLIDS; SORTING
- B07B—SEPARATING SOLIDS FROM SOLIDS BY SIEVING, SCREENING, SIFTING OR BY USING GAS CURRENTS; SEPARATING BY OTHER DRY METHODS APPLICABLE TO BULK MATERIAL, e.g. LOOSE ARTICLES FIT TO BE HANDLED LIKE BULK MATERIAL
- B07B13/00—Grading or sorting solid materials by dry methods, not otherwise provided for; Sorting articles otherwise than by indirectly controlled devices
- B07B13/14—Details or accessories
- B07B13/16—Feed or discharge arrangements
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/0896—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid particle transport, separation: process and apparatus
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Combined Means For Separation Of Solids (AREA)
- Glanulating (AREA)
- Feeding, Discharge, Calcimining, Fusing, And Gas-Generation Devices (AREA)
- Joints Allowing Movement (AREA)
- Nonmetallic Welding Materials (AREA)
- Steroid Compounds (AREA)
- Friction Gearing (AREA)
- Electric Connection Of Electric Components To Printed Circuits (AREA)
- Powder Metallurgy (AREA)
Abstract
Spherical balls, notably microballs of welding alloys, are produced by passing a melted material through vibrating orifices (8) of a granulation pot (4), in order to form droplets which solidify when falling, by gravity, into a cooling tower (16) filled with an inert gas. To improve the surface condition of the balls, the inert gas comprises approximately 15 to 150 ppm of oxygen. Moreover, the melted material is subject to ultrasound stirring (21, 22) just before being fed into the granulation pot. The balls are, preferably, dampened at the outlet of the cooling tower by brushes (25) composed of polyamide wires. Besides, the control of the vibration frequency of the vibrating orifices in relation to the percentage of balls meeting the standards enables to improve the output.
Description
Technical field
The present invention relates to produce the equipment of ball (spherical ball), comprising:
Be used for the material that the manufacturing ball is used is supplied to the device of melting vessel,
Second container that is communicated with melting vessel, with the reception melted material,
Pass through the device that at least one nozzle forms jet by the melted material that is contained in second container,
Oscillation device is used for vibration is passed to nozzle, so that jet is changed into drop,
Cooling tower, it is arranged on the exit of nozzle and has been full of inert gas, and wherein the droplet solidification that descends because of gravity forms ball, and
The device that is used to receive ball in the lower end of cooling tower.
Background technology
Existing big metering method and the Granulation Equipments that is applied to multiple industrial circle for example is used in metallurgy, fertilizer, food or the pharmaceuticals industry etc.Their purpose all is material is transformed balling-up, and this material is fusion, has low viscosity, surface of good tension force, the good flowable that passes through nozzle in open air or under neutral gas, and is easy to solidify by cooling.
For exemplary purposes, the document WO-A-8101811 corresponding to No. the 4428894th, United States Patent (USP) has described the method and apparatus of producing the metallic particles of 0.1 to 5mm diameter from pool of molten metal.According to this known method, form the motlten metal jet, jet is divided into independently drop, this drop is caused falling from fluid by inert gas atmosphere because of gravity this jet, so that drop is frozen into particle by cooling through the vibration nozzle.
Yet, almost do not have the Granulation Equipments of method and calibration can have the ball that good output ground large-scale production has the size homogeneous of fabulous surface state in the practice.In addition, be which kind of material (organic articles, metal ...) no matter by this technology granulation, usually generation is, the ball of gross distortion or the ball that is sticked together (usually being paired) account for the certain proportion of output, and a pair of like this ball is known as dumbbell body (dumbbell).
For application-specific, also need to produce ball, microballoon more specifically, this ball do not have any blemish and have very accurate granularity.Preferably, these tiny balls not only must have consistent diameter, and must be desirable spherical and be discrete.In mechanical industry, when ball was made of the material with higher hardness, people adopted selecting device or sorting unit usually, comprised funnel, yardage roll etc.Particularly under the situation of ball as bearing, nib etc.Under the situation that cause speckle can not for the ball surface, keep pellet impact and friction then.Otherwise in some cases, the sphericity of ball and surface state should not be selected device and change.
Especially, form the welding alloy ball that connects in the electronics industry, more have this situation, for example be used for the situation of BGA type (" BGA " (Ball Grid Array)) for being used in.Have, the metal that is used for welding alloy is the soft metal again, and the surface state of the ball of this metalloid formation very easily changes.
Summary of the invention
The objective of the invention is to obtain not have the ball of any blemish.More particularly, ball must be desirable spherical, has fabulous surface state, and without any oxidation.The composition of ball must be in every batch of product stabilizer poles all, and the granularity tolerance is minimum.
According to the present invention, this purpose is reached in such equipment, this equipment comprises the downstream chamber in the melting vessel, be used for before metal material transmits second container into, the melted material that is contained in the downstream chamber being carried out the device that ultrasonic wave stirs, and the inert gas in the cooling tower contains scheduled volume oxygen.
According to progress of the present invention, the device that receives ball comprises device for impact absorbing.Preferably, described device comprises the brush that is made of the polyamide-based silk thread, and the orbit-shaped of the ball in brush and the cooling tower is into about the angle of 45 degree.In addition, the fabric yardage roll can be arranged on the inner rim of cooling tower inwall on the brush.
According to a preferred embodiment, this equipment comprises in the cooling tower exit and being used for the regular device of discharging of ball, and comprises the robot scaling equipment (calibrationmeans) that is used for napiform root is become according to its size separation three classes.This equipment also comprises: the device that the every class ball that obtains in each discharge process is weighed; The information that provides according to weighing device determines to satisfy the device of percentage of the ball of preassigned; And, regulate the device of oscillation device frequency with respect to described percentage.
Another object of the present invention provides a kind of equipment that takes out ball, and this equipment has the ball sorting unit, and this sorting unit can sort out the ball of diameter homogeneous, not being that desirable spherical ball puts aside with all.
According to the present invention, this purpose is by following true the realization, promptly, sorting unit comprises and is used for ball is supplied to device on first inclined plane on the inclined plane in succession of being separated by the interval of pre-sizing, takes this at least the first inclined plane and have the surface of its roughness greater than the roughness on subsequently inclined plane on the direction of displacement of ball.
According to a preferred embodiment, be used for the device that ball is provided on first inclined plane is comprised rolling surface, retention device, will rest in the catapult-launching gear that the ball on this retention device ejects from rolling surface with jolting.
Preferably, catapult-launching gear comprises hollow tilting gearing (ramp), and this tilting gearing is by horizontal moving forward and backward excitation and be equipped with a plurality of air ejectors that are evenly distributed along tilting gearing.
According to another characteristic of the invention, be used for the device that ball supplies on first inclined plane is comprised conveyer belt that this conveyer belt has the inclined surface consistent with this inclined plane direction, and have the opposite direction of rotation of direction of on described surface, rolling with ball.
Another object of the present invention relates to the removal of the ball that is sticked together.
According to progress of the present invention, this another purpose is by following true realization, that is, sorting unit comprises gear in the downstream, inclined plane, this gear is by encouraging around rotatablely moving of sloping shaft and comprising that longitudinal groove, the size of this groove can make the ball of separation roll and prevent that the adhesion ball is to rolling.
Description of drawings
From following that provide for the example purpose, be not that limit it and the explanation of specific embodiments of the invention illustrated in the accompanying drawings, other advantage and feature can more clearly manifest, in the accompanying drawing:
Fig. 1 is the schematic cross sectional views according to the specific embodiment of equipment of the present invention;
Fig. 2 illustrates in greater detail the lower part according to the granulation crucible of the equipment of Fig. 1;
Fig. 3 illustrates in greater detail the specific embodiment according to the outlet opening of the granulation crucible of Fig. 2;
Fig. 4 is the cutaway view of edge according to the line A-A of the crucible of Fig. 1;
Fig. 5 has shown the specific embodiment that is arranged on according to the device for impact absorbing of the cooling tower lower part of the device of Fig. 1;
Fig. 6 is the cutaway view along the line B-B of the device for impact absorbing of Fig. 5;
Fig. 7 has schematically shown and has been arranged on according to the calibration in the cooling tower exit of the equipment of Fig. 1 and the specific embodiment of weighing device;
Fig. 8 has schematically shown the specific embodiment according to the sorting unit of present device;
Fig. 9 and 10 shows in detail the specific embodiment that is positioned at according to the device part of the inclined plane upstream end of the selecting device of Fig. 8 respectively, is respectively side view and bottom view;
Figure 11 shows the specific embodiment according to the outlet rolling surface of the funnel of the device of Figure 10, and this figure is from the free end of rolling surface;
Figure 12 and 13 shows the outlet rolling surface position for the movable inclined device of two extreme positions of tilting gearing and funnel;
Figure 14 shows gear according to the sorting unit of Fig. 8 with cutaway view; And
Figure 15 shows the layout of blocking in according to a pair of ball in the groove of the gear of Figure 14.
The specific embodiment
Equipment according to Fig. 1 comprises by the container or the crucible 1 of any appropriate device (not shown) heating, wherein can inject the material that is used for ball that is the solid alloy form by supply lock (supply lock) 2.The material that injects with billet, ingot or bar 3 forms is in the melting vessel fusion.The also bottom that is connected to crucible 1 by at least one transfer tube 5 in its bottom by second container or the granulation crucible (granulation pot) 4 of any appropriate device (not shown) heating.Tube connector 6 connects the top of crucible 1 and 4 above melted material horizontal plane 7, thereby the gaseous environment pressure P above the melted material is identical in two crucibles.In addition, horizontal plane detector (not shown) is connected to the ingot feeding system, and is constant with the horizontal plane that keeps melted material in the crucible 1 and 4.
Granulation crucible 4 comprises at least one nozzle with predetermined diameter 8 usually in its underpart, molten alloy flows out by the form of this nozzle with jet (jet).The oscillator 9 that is fixed on granulation crucible 4 lids passes to nozzle 8 by vibration supporting plate 10 with vibration, and this vibration is by the vertical excitation that seesaws.Be well known that vibration supporting plate 10 is connected to oscillator 9 by metallic rod 11, oscillator for example is an electromagnetic type, and this metallic rod is passed the lid 12 of granulation crucible 4 through slype.Frequency of oscillation changes between 200 hertz to 10000 hertz, preferably between 200 hertz and 6000 hertz.
Material such as the weld metal alloy is melted in the crucible 1, is transferred in the granulation crucible 4 by transfer tube 5 with liquid form then.Gaseous environment (as the nitrogen) pressure P of melted material top is able to measure enduringly and regulate by control circuit 13, so that provide pre-set velocity (according to nozzle diameter preferably between 0.5 and 5 meter per seconds) for the melted material jet of each nozzle 8 of passing granulation crucible bottom.The vibration of vibration supporting plate 10 is passed to laminar jet 14 from nozzle 8.As shown in Figure 2, jet 14 is divided into drop 15 then, and the diameter of drop is mainly determined (preferably changing) by the diameter D of nozzle 8 in 80 to 800 microns scope.Drop is full of because of gravity drops in the cooling tower 16 of inert gas, and they are frozen into ball in this cooling tower.Can make ball in for example cooling fast in 2 to 3 seconds in use as helium under the downforce, this pressure promptly 30 millibars and greater than 100 millibars between, preferably about 50 millibars, preferably ± 1 change in millibar the scope.The height of cooling tower 16 is generally several meters, for example 7 meters.Certainly adopt other inert gas.Yet the use of nitrogen or argon gas means that the use of cooling tower is up to about twice.
One or several diameter is that the round nozzle 8 of D is preferably formed by such material, and the melted material that this material can not passed wherein soaks into, and the surface tension of this material has been offseted the surface tension with the material of granulation.For example purposes, nozzle 8 is made by sapphire or ruby.In Fig. 2 and 3 described specific embodiments, the wall of granulation crucible 4 17 is made by stainless steel, and comprises sapphire or the ruby inserts 18 that wherein is formed with a nozzle 8 at least in its underpart.Each nozzle 8 is limited by the upstanding wall that height H is less than or equal to diameter D.In a preferred embodiment, D=450 micron, H=190 micron.In the specific embodiment of Fig. 2 and 3, nozzle 8 is upwards tapered in its underpart, and at this place, bottom, nozzle is limited by the inclined wall or the curved wall 19 of inserts 18.
According to the present invention, crucible 1 comprises downstream chamber 20, and melted material is subjected to the ultrasonic wave stirring in this downstream chamber.This stirring can realize that this oscillation device for example is piezo-electric type (piezzo-electric type) by the bar 21 that is immersed in the melted material that is contained in the downstream chamber 20 and encourage because of vertically seesawing of oscillation device 22.This ultrasonic wave with the frequency that for example changes between 20 kilo hertzs and 30 kilo hertzs stirs, and can improve the surface state of ball greatly.This stirring can not be carried out in granulation crucible 4, because it may disturb melted material to pass through flowing of nozzle 8.This stirring mainly is to cause melted material to homogenize before injecting granulation crucible 4.This stirring is only carried out in downstream chamber 20, that is, and and near being positioned at the melted material outlet of granulation crucible 4 of crucible 1, and in the part of whole material fusion wherein.
In preferred embodiment shown in Figure 4, the volume of downstream chamber 20 is less than about 20% of the volume of crucible 1.Can crooked wall 23 define the downstream chamber 20 in the crucible 1.Wall 23 is equipped with the passage 24 of several millimeters (as 5 millimeters) in its underpart, so that melted material can enter the downstream chamber.
Dispersion that melted material homogenizing before it injects granulation crucible 4 causes nucleus (crystallisation germ) simultaneously and minute impurities are in the suspension of melted material in advance, this may disturb melted material to pass through flowing of nozzle 8, says nothing of and has blocked described nozzle.
Can notice that do not comprise that the device fabrication that this ultrasonic wave stirs goes out the ball that may comprise the pit of the different size and the degree of depth in its surface, these pits make that ball is not suitable for being used in the electronics industry.Stir according to ultrasonic wave according to the present invention and to make and significantly to reduce this class defective, usually even make this class defective complete obiteration.Supersonic oscillations can be carried out enduringly.Also can only carry out off and on by control circuit 13.Should be noted that, melted material can be from the downstream chamber 20 be carried to granulation crucible 4 continuously, and the effect that homogenizes is reflected on the surface state of ball, even melted material must be by keeping dormant state one special time in granulation crucible 4 before the nozzle 8, for example, up to 30mn.
The another kind of method that can improve the surface state of gained ball comprises the character operation by the gas that contains in the cooling tower 16.In fact, described character is of crucial importance for sphericity, its rapid solidification and its surface state of ball.According to a further aspect of the invention, the oxygen of scheduled volume is injected in the inert gas of cooling tower 16, the amount of this oxygen is preferably several ppm, and for example about 15 to 150ppm.Inert gas at cooling tower lacks under the situation of oxygen, and club has a plurality of small (micro-facet) on its surface, if oxygen is injected into this facet in the inert gas then can disappears.Yet if amount of oxygen is excessive, ball does not just always have desired sphericity.
The ultrasonic wave of melted material in the downstream chamber homogenizes and scheduled volume oxygen injected the surface state maximization, the particularly tiny balls of being made by the weld metal alloy that combining of cooling tower can make ball.
Ball is preferably cushioned in the reception of cooling tower 16 lower ends, to avoid any variation of ball surface state.In the known device of majority, ball is received in the liquid.It is to need ball dry in the step in the back that this class receives shortcoming.
In the preferred embodiment shown in Fig. 5 and 6, impact basically by brush 25 absorptions.It can eliminate any liquid in the reception area, and all stages of processing all carry out under drying condition.Each brush 25 is made of the polyamide-based silk thread, and an end of brush is fixed on the bottom upstanding portion of cooling tower inwall and receives near the junction of awl 26.The track of ball forms the angle of about 45 degree in silk thread and the cooling tower,, becomes miter angle with vertical line basically that is.In one embodiment, about 10 centimetres four the paired relative brushes 25 of width are along the circumferential distribution of cooling tower, and the free end of the silk thread of two relative brushes is above another.The diameter of silk thread is less than the diameter of ball.In case impact to be absorbed, the pliability of brush concede points by, and do not change its surface state.
Ball can utilize yardage roll (roller) 27 to finish by the impact absorption of brush 25 before arriving reception area 26, and this yardage roll is preferably made by the polyamide-based fabric, is arranged on the lower periphery of cooling tower inwall, was positioned at the brush top.Can cover the zone that is right after the brush top by vertically disposed yardage roll 27 (Fig. 5 and 6).Ball also can cushion thus to any impact of cooling tower inwall, and this impact may be caused on brush 25 by the ball bullet.
The reception area 26 of cooling tower extends from lock (lock) 28, and this lock is provided with inlet valve 29 and the outlet valve of handling by control circuit 13 30.This lock makes the ball that accumulates in the reception area 26 regularly to discharge.Described then ball is transferred to scaling system (calibration system).
In the specific embodiment of Fig. 7, the ball of discharge (usually 100 and 300g/mn between) drop on because of gravity on the top sieve 31, this sieve does not allow size pass through greater than the ball of preassigned.The ball by top sieve 31 falls on bottom sieve 33 by first funnel 32, and the bottom sieve allows too small ball to pass through.Described ball falls into first groove 35 by second funnel 34.Standard compliant ball is retained in the bottom sieve 33.By turn sieve 31 and 33, excessive ball and standard compliant ball are fallen, through the 3rd funnel 36 and the 4th funnel 37, enter second groove 38 and the three-flute 39 respectively respectively.Thus, napiform root is divided into three classes according to its size: satisfactory ball enters three-flute 39, and too small ball enters first groove 35, and excessive ball enters second groove 38.
Take out circulation for each, first, second and the 3rd balance 40,41 and 42 that are placed on first, second and three-flute 35,38 and 39 belows respectively provide representative to collect the signal M of the weight of the ball in first, second and the three-flute respectively to control circuit 13
1, M
2And M
3Control circuit 13 is determined the percentage of the standard compliant ball of discharge according to this weight information, and acts on the granulation parameter to keep the output near 100%.In a preferred embodiment, the frequency of control circuit 13 special controls and adjusting oscillator 9.In fact, the frequency increase of oscillator 9 tends to make the ball size to reduce.For exemplary purposes, for the rated frequency of 500 hertz oscillators, variation can reach ± and 5 hertz.
The invention still further relates to the equipment that takes out ball, this equipment has the ball sorting unit of the ball of selection diameter homogeneous, not being that the ball of full spherical puts aside with all.
Proposed by inclined plane selection different-diameter or had the spherical artefact of remarkable distortion, and the velocity sorting ball that reaches at different balls.
This class sorting is suitable for the such ball of sorting, and promptly all balls had had the little same diameter of tolerance before point selection operation, but their sphericity changes in than close limit.The purpose of point selection operation is that to eliminate all be not full spherical and the faulty ball of its surface state.
In the embodiment shown in fig. 8, equipment comprises the groove that is hopper 43 shapes, wherein placed will sorting ball.This groove is arranged on the equipment exit, is used to take out above-mentioned ball.Ball is in succession through inclined plane 44a, 44b, 44c, 44d.Each inclined plane is positioned at the below slightly on previous inclined plane, and horizontal interval e1 separates two continuous inclined planes.Interval between each inclined plane can be removed and be arrived beveled end portion, and does not reach the ball of enough speed, with through subsequently inclined plane, and does not fall in succession between the inclined plane.
All inclined planes all do not have identical surface state, and this surface is controlled ideally with respect to each sphere diameter that will sorting.In fact, the speed of ball depend on cooperation usefulness, particularly gravity, frictional force, the air force load of several loads, with the interaction of rolling surface etc.The inclined plane is preferably made by metallic plate, and its surface has controlled roughness on the displacement of ball direction, and this roughness is bigger at least one first inclined plane.The roughness of the first inclined plane 44a has the ball of blemish greater than the roughness on subsequently inclined plane so that slow down more significantly.Along with this ball shows track from the teeth outwards, it is complicated more really obviously to cut defective, and this makes this ball slow down, and causes ball for example falling between inclined plane 44a and the 44b.The existence of controlled roughness should not cause friction to increase, but with respect to the unevenness of ball its track is come and go, and this friction may cause the surface state of ball to descend.This makes sphere can follow more straight track, and therefore reaches higher muzzle velocity.
In order to obtain desired roughness, handle by any suitable means on the surface on inclined plane, for example by frosted, impact (shot-peening) or by any other machinery and/or chemical means, perhaps by suitable coating covering etc.In a preferred embodiment, all have can be less than the high roughness on second inclined plane for the first inclined plane 44a and 44b.The inclined plane 44d in back (may be latter two inclined plane 44c and 44d) can have desirable smooth surface.So the interaction between the surface state on ball blemish and inclined plane can be removed incomplete ball fast.
Interval between the gradient on each inclined plane and two the continuous tilt faces determines with respect to the diameter of ball, make ball with fabulous sphericity with enough from an inclined plane through and the speed that arrives next inclined plane is rolled on the inclined plane.The bending that comprises is upwards distinguished on each inclined plane at its upstream, the impact when on the inclined plane, receiving ball of being used to decay, and prevent the ball bounce-back.
For exemplary purposes, in order to choose its diameter usually less than 500 microns welding alloy microballoon, each inclined plane has on floor projection and can be about 10 to 15 centimetres length L and can be 1 meter width.Perpendicular separation e2 between two continuous tilt faces can be less than or equal to 1 centimetre, and horizontal interval e1 can be about 1 centimetre to 3 centimetres.The number on inclined plane and ball size are inversely proportional to, and preferably change at 2 to 5 interblocks.In addition, ball is heavy more, then advances soon more.Thereby the angle on inclined plane must be little, can carry out good choosing.
Ball from hopper 43 supplies on the first inclined plane 44a by rolling surface (rolling plane) 45, and this rolling surface tilts a little, extends from the bottom of funnel 43.Ball comes out by slype 46 under the effect of gravity in the bottom of funnel 43, to form one deck roller ball on rolling surface.At the free end of rolling surface 45, ball rests on the block piece 47.Among Fig. 8 to 10, block piece 47 is made of the cylinder on the whole at least width that is arranged on rolling surface 45, and this cylinder is perpendicular to the flow direction of ball on the rolling surface 45.Therefore alignment before block piece 47 of ball.Separate with block piece 47 less than the interval of bulb diameter free end rolling surface 45.
The ball that aligns in block piece 47 the place aheads is being run from rolling surface and is being ejected.This ejects preferably and realizes that by tilting gearing 48 this tilting gearing is made of hollow pipe, and wherein compression drying air or inert gas (nitrogen, argon gas etc.) stream in continuous-flow.Tilting gearing 48 is parallel to the free end that block piece 47 is arranged on rolling surface 45.It comprises the air nozzle 49 at the interval of determining between a plurality of sensing rolling surface free ends and the block piece, this air nozzle evenly distributes and the formation catapult-launching gear along tilting gearing 48, and this catapult-launching gear is used to raise delegation's ball that (ground preferably jolts) aligns before block piece 47.
In order to ensure the ejection of jolting of ball, tilting gearing 48 is driven by snap switch (jack) (not shown), and it has laterally seesawing perpendicular to the flow direction of ball on the rolling surface 45 (among Figure 10,12 and 13 from left to right).Each position for the tilting gearing 48 and the rolling surface 45 of two extreme position in the process that seesaws of tilting gearing has been shown in Figure 12 and 13.Rolling surface 45 comprises thickness uniformly from being leg-of-mutton barrier 50 (Figure 11) at its free end at least, and this barrier is divided into the little passage of a plurality of width 51 with described face.Barrier 50 stretches out very slightly at the free end of rolling surface.The bottom of triangular-section that is parallel to the free-ended barrier 50 of rolling surface 45 has length l 1, and the summit partition distance l2 (Figure 12) of two adjacent barriers.The displacement (Figure 12 and 13) of the air nozzle 49 that the base angle of triangle barrier 50 has been determined in two extreme positions of tilting gearing 48.
Therefore, at the end of stroke, when tilting gearing 48 in these two terminal positions located, all air nozzles 49 were positioned at the below of the end of barrier 50.Then, the gas jet of coming out from tilting gearing 48 by air nozzle 49 is directed into barrier 50 belows, and can not eject the ball that is placed in 45 upper channels 51 of rolling plane.On the contrary, during tilting gearing 48 displacements, delegation's ball that the air-flow that comes out from the air nozzle relevant with each passage causes resting on the block piece 47 ejects.Ejection is progressive, with the displacement synchronous of air nozzle.Tilting gearing intermittently launches on the time of staying at the two ends ground of can realizing jolting, and thoroughly cleaning downstream space and restriction are easy to change interaction between the ball of its surface state before new delegation's ball ejects thus.Therefore ball amount on each scrollable area is regulated and is limited.
In the preferred embodiment of Fig. 8, barrier defines 7 passages 51.The length l 1 of the triangular base of barrier 50 can be about 20 to 30 millimeters, is about 130 millimeters apart from l2.Tilting gearing continues for example in (frequency range is between 0.1 and 1 hertz) variation between 1 second and several seconds the displacement between two extreme position.
The ball that ejects is by 52 guiding of the reflecting plate (baffle) on conveyer belt 53 inclined planes.Preferably be the reflecting plate 52 of curved shape and the passage that block piece 47 defines the ball that is used to eject, this ball is fallen on the inclined plane of the conveyer belt 53 that is arranged on the assembly below that is made of rolling surface 45, block piece 47, tilting gearing 48 and reflecting plate 52 then.Fall to having the conveyer belt surface of the ball of ejection to tilt on it in the direction identical with inclined plane 44a to 44d.The direction of rotation of conveyer belt 53 be conveyer belt should the surface on the rightabout (Fig. 8) of direction of the bowl.
Ball with good sphericity rolls towards the first inclined plane 44a on the conveyer belt inclined surface.The selection of the velocity of displacement of conveyer belt makes the ball that rolls on its displacement rightabout on its inclined surface arrive first inclined plane.For exemplary purposes, the speed of conveyer belt can be preferably 2m/mn for about 0.5 to 5m/mn.Conveyer belt carries out the first time and selects.In fact, towards the rear portion emptying and fall into first groove 54, and the ball with sphericity is rolled into first inclined plane in the opposite direction by conveyer belt for can not roll or roll on the conveyer belt inclined surface too slow ball with big blemish or binary ball.
The outlet of an inclined plane 44d in the end, the ball of choosing falls into funnel 55.Active belt 56 can be arranged between last inclined plane 44d and the funnel 55, before in receiving funnel, does last the selection between ball.Among Fig. 8, active belt 56 comprises the top edge that connects two walls, and one of them wall is ball guide funnel 55 faster, and another wall is discharged slower ball, and this ball falls into the top edge upstream.
The above-mentioned selecting device surface state of ball is relatively chosen the uniform ball of diameter.The ball that only has the ideal surfaced state could arrive funnel 55.Yet the ball that may stick together arrives the situation of funnel 55.In the practice, in about 1,000,000 balls, the ball of 2 or 3 pairs of adhesions arrives funnel.Drop on the conveyer belt 53 at a pair of adhesion ball 60, especially like this, make the rolling of paired ball can not slow down when dropping on the different inclined planes then, for example as the symmetrical longitudinal axis S (Figure 15) of paired ball during fully perpendicular to the direction of the displacement of ball.Also in order to eliminate the adhesion ball that may arrive funnel 55, this equipment has preferably increased the effective diameter that is arranged on the downstream, inclined plane and for example has been about 30 centimetres gear 57.
In the specific embodiment of Fig. 8, funnel shaped funnel 55 makes ball flow on the top of gear 57.Described gear encourages by centering on slowly rotatablely moving of sloping shaft 8, and comprises longitudinal groove 59, and the size of this longitudinal groove makes segregate ball can roll and prevent ball 60 rollings (Figure 14 and 15) of a pair of adhesion.Flawless ball rolls in the groove 59 of gear, and collects to advance to be arranged in second groove 61 in gear downstream.Be blocked in the groove this to ball 60 of adhesion with gear around axis 58 rotations, and rotated half-turn when gear, and wherein be placed with this groove when having arrived the gear bottom of three-flute top, because of gravity falls into three-flute 62 ball 60.
Preferably, gear 57 comprises a hundreds of groove.The bottom of groove 59 is about 1.2 to 1.5 times of bulb diameter, makes the ball of a pair of adhesion not place and to roll in the described groove perpendicular to groove.For making ball be easier to roll in the groove 59, preferably, the tip of little circle is worn on the summit of gear teeth.
Can place perpendicular to groove 59 with the reflecting plate (not shown) that is circular shape of outside diameter of gear coupling, under the situation of the exit of funnel 55 generation bottleneck, to be used as barrier.
Specific embodiment shown in the present invention is not limited to.Especially, the number of nozzle 8 can be with shown in the drawings different with layout.Similarly, in the sorting of the ball in cooling tower exit with weigh and can be undertaken by any suitable means, these means can be separated the ball that satisfies standard with other ball, desired information can also be provided.The number of sieve, funnel and groove can be with shown different with layout.Preferably, control circuit 13 receives the signal of the various parameters of representative, and described parameter is easy to the ball by this device fabrication is exerted an influence, and this circuit is also controlled the various parts that may influence described parameter.Especially, except signal M
1, M2 and M
3Outward, it is also via pressure P in any proper device reception crucible 1 and granulation crucible 4 and the cooling tower 16 and the measuring-signal of temperature θ.Especially, it has controlled material 3 from supplying with infeeding of lock 2, the air pressure in the taking-up of ball by lock 28, oscillation device 22, oscillator 9, crucible 1 and 4 heating, crucible and the cooling tower, and be included in amount of oxygen in the cooling tower.
The shape on the inclined plane of selecting device, size, layout and number can be suitable for the size of the ball that will choose.Block piece 47 needs not to be columniform.Because sharp edges may be damaged the surface state of ball, so that curved shape is still is favourable.
Claims (19)
1. equipment of producing ball comprises:
The material that is used for being used for making ball is supplied to the device of melting vessel (1);
Second container (4) that is communicated with melting vessel (1) is to receive melted material;
Pass through the device that at least one nozzle (8) forms jet (14) by the melted material that is contained in second container;
Oscillation device (9,10,11) is used for vibration is passed to nozzle (8), so that jet (14) is transformed into drop (15);
Cooling tower (16), it is arranged on the exit of nozzle (8) and has been full of inert gas, and the drop (15) that falls because of gravity solidifies therein and forms ball; And
Be used for receiving the device of ball in the lower end of cooling tower (16),
It is characterized in that, this equipment comprises the downstream chamber (20) in the melting vessel (1) and is used for transmitting at melted material that second container (4) carries out the device (21,22) that ultrasonic wave stirs to the melted material that is contained in downstream chamber (20) before, and the inert gas that contains in the cooling tower (16) contains the oxygen of scheduled volume.
2. equipment as claimed in claim 1 is characterized in that, is included in amount of oxygen in the inert gas of cooling tower (16) and is about 15 to 150ppm.
3. as a described equipment in claim 1 and 2, it is characterized in that the volume of downstream chamber (20) is less than about 20% of the volume of melting vessel (1).
4. as each the described equipment in the claim 1 to 3, it is characterized in that melting vessel (1) comprises the wall (23) that limits downstream chamber (20), described wall (23) is furnished with passage (24) in its underpart, so that melted material can enter downstream chamber (20).
5. as each the described equipment in the claim 1 to 3, it is characterized in that the ultrasonic wave agitating device comprises in the melted material that is immersed in the downstream chamber and by the bar (21) of the vertical excitation that seesaws.
6. as each the described equipment in the claim 1 to 5, it is characterized in that nozzle (8) is made by the material that can not be melted the material infiltration.
7. as each the described equipment in the claim 1 to 6, it is characterized in that the device that is used to receive ball comprises device for impact absorbing.
8. equipment as claimed in claim 7 is characterized in that, device for impact absorbing comprises the brush (25) that is made of the polyamide-based silk thread, and the orbit-shaped of the ball in this brush and the cooling tower (16) is into about miter angle.
9. equipment as claimed in claim 8 is characterized in that, device for impact absorbing comprises the fabric yardage roll (27) on the lower periphery that is arranged on brush (25) top cooling tower (16) inwall.
10. as each the described equipment in the claim 1 to 9, it is characterized in that, exit in cooling tower (16) comprises the device (28,29,30) and the robot scaling equipment that are used for regularly discharging ball, and this robot scaling equipment comprises the device (31,33) that is used for relative its size separation of ball is become three classes.
11. equipment as claimed in claim 10 is characterized in that, it comprises the device (40,41,42) that all balls of each class that obtains are weighed, the information (M that basis is provided by weighing device in each discharge process
1, M
2, M
3) determine to satisfy the device (13) of percentage of ball of preset standard and the device that is used for regulating the frequency of oscillation device (9) with respect to described percentage.
12. as each the described equipment in the claim 1 to 11, it is characterized in that, it comprises sorting unit, this sorting unit comprises and is used for ball is supplied to device on first inclined plane (44a) on the inclined plane in succession (44a, 44b, 44c, 44d) of being separated by the interval (e1, e2) of pre-sizing, and at least the first inclined plane (44a) has the surface of its roughness greater than the roughness on subsequently inclined plane on the direction of displacement of ball.
13. equipment as claimed in claim 12 is characterized in that, last at least inclined plane (44d) has perfectly smooth surface.
14. as a described equipment in claim 12 and 13, it is characterized in that, be used for ball is supplied to the catapult-launching gear (48,49) that device on first inclined plane comprises rolling surface (45), retention device (47), makes the ball that rests on this retention device jolt and eject from rolling surface.
15. equipment as claimed in claim 14 is characterized in that, catapult-launching gear comprises hollow tilting gearing (48), and this tilting gearing is by laterally moving forward and backward excitation and being equipped with a plurality of along the equally distributed air ejector of tilting gearing (49).
16. as each the described equipment in the claim 12 to 15, it is characterized in that, be used for the device that ball supplies on first inclined plane (44a) is comprised conveyer belt (53), this conveyer belt have the inclined surface consistent with the inclined plane direction and with ball in the opposite direction of rotation of described lip-deep rotating direction.
17. equipment as claimed in claim 16 is characterized in that, is used for the device that ball is provided on first inclined plane (44a) is comprised reflecting plate device (52), the ball that launches with guiding is to the inclined surface of conveyer belt (53).
18. as each the described equipment in the claim 12 to 17, it is characterized in that, the downstream of (44a, 44b, 44c, 44d) comprises gear (57) on the inclined plane for it, this gear is by encouraging around rotatablely moving of sloping shaft (58) and comprising that longitudinal groove (59), the size of this groove can make the ball of separation roll and prevent that the adhesion ball from rolling to (60).
19. equipment as claimed in claim 18, it is characterized in that, it comprises the first receiving device (61) of the indefectible ball of the groove (59) that is used for tumbling gear (57), and in the rotary course of gear (57), the adhesion ball that is blocked in the groove (59) falls into second receiving system (62) to (60) because of gravity.
Applications Claiming Priority (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR0110007A FR2827793B1 (en) | 2001-07-26 | 2001-07-26 | DEVICE FOR PRODUCING SPHERICAL BALLS |
| FR0110007 | 2001-07-26 | ||
| FR0110702 | 2001-08-10 | ||
| FR0110702A FR2828418B1 (en) | 2001-08-10 | 2001-08-10 | SPHERICAL BALL SELECTION DEVICE |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1400073A true CN1400073A (en) | 2003-03-05 |
| CN1197674C CN1197674C (en) | 2005-04-20 |
Family
ID=26213117
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB021270422A Expired - Fee Related CN1197674C (en) | 2001-07-26 | 2002-07-26 | Pellet producing apparatus |
Country Status (11)
| Country | Link |
|---|---|
| US (1) | US6676890B2 (en) |
| EP (1) | EP1279450B1 (en) |
| JP (1) | JP4118626B2 (en) |
| KR (1) | KR100866294B1 (en) |
| CN (1) | CN1197674C (en) |
| AT (1) | ATE433815T1 (en) |
| CA (1) | CA2393862A1 (en) |
| DE (1) | DE60232622D1 (en) |
| MY (1) | MY127347A (en) |
| SG (1) | SG103876A1 (en) |
| TW (1) | TW577780B (en) |
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| CN101844229A (en) * | 2010-03-24 | 2010-09-29 | 峨嵋半导体材料研究所 | Preparation method and production equipment of high-purity antimony particles |
| CN105170022A (en) * | 2014-06-16 | 2015-12-23 | 新特能源股份有限公司 | Granulation apparatus, preparation method for preparing catalyst for silicon tetrachloride catalytic hydrogenation reaction, and silicon tetrachloride catalytic hydrogenation reaction method |
| CN106714955A (en) * | 2014-09-29 | 2017-05-24 | 卡萨尔公司 | Apparatus and method for prilling a liquid, preferably urea melt |
| WO2019024419A1 (en) * | 2017-08-04 | 2019-02-07 | 米亚索乐装备集成（福建）有限公司 | Atomization device and method for preparing metal alloy powder |
| CN110054396A (en) * | 2018-01-18 | 2019-07-26 | 宁波大学 | A kind of 2S2G chalcogenide glass microballoon producing device |
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| CN114057487A (en) * | 2021-12-14 | 2022-02-18 | 中钢集团南京新材料研究院有限公司 | Isostatic pressing graphite preparation device and preparation method |
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| CN100395040C (en) * | 2005-12-08 | 2008-06-18 | 安徽精通科技有限公司 | Method for projecting and screening microelectronic-packed tin ball |
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| FR2471827A1 (en) * | 1979-12-21 | 1981-06-26 | Extramet Sa | DEVICE FOR THE PRODUCTION OF UNIFORM METAL PELLETS |
| DE3538267A1 (en) | 1984-12-21 | 1986-06-26 | Rudolf Dipl.-Ing. 4048 Grevenbroich Koppatz | METHOD AND DEVICE FOR PRODUCING METAL GRANULES |
| JPS61221310A (en) * | 1985-03-26 | 1986-10-01 | Agency Of Ind Science & Technol | Method and apparatus for producing pulverous powder of metal or alloy or the like |
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| US5229016A (en) * | 1991-08-08 | 1993-07-20 | Microfab Technologies, Inc. | Method and apparatus for dispensing spherical-shaped quantities of liquid solder |
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| JP2000328111A (en) * | 1999-05-14 | 2000-11-28 | Nippon Steel Corp | Manufacture of small metal ball, and device therefor |
| JP2000328112A (en) | 1999-05-24 | 2000-11-28 | Sumitomo Metal Mining Co Ltd | Manufacture of solder ball and manufacturing device therefor |
| US6312498B1 (en) * | 1999-12-14 | 2001-11-06 | Mk Electron Co., Ltd. | Method of manufacturing solder balls |
| JP2001226706A (en) * | 2000-02-15 | 2001-08-21 | Hitachi Metals Ltd | Apparatus for manufacturing fine metallic ball |
| JP2001254108A (en) * | 2000-03-14 | 2001-09-18 | Hitachi Metals Ltd | Manufacturing method and manufacturing apparatus for fine metal ball |
| US6491737B2 (en) * | 2000-05-22 | 2002-12-10 | The Regents Of The University Of California | High-speed fabrication of highly uniform ultra-small metallic microspheres |
| TW577780B (en) * | 2001-07-26 | 2004-03-01 | Ind Des Poudres Spheriques | Device for producing spherical balls |
-
2002
- 2002-07-10 TW TW091115330A patent/TW577780B/en not_active IP Right Cessation
- 2002-07-12 SG SG200204286A patent/SG103876A1/en unknown
- 2002-07-15 US US10/194,011 patent/US6676890B2/en not_active Expired - Fee Related
- 2002-07-17 CA CA002393862A patent/CA2393862A1/en not_active Abandoned
- 2002-07-19 AT AT02354113T patent/ATE433815T1/en not_active IP Right Cessation
- 2002-07-19 MY MYPI20022736A patent/MY127347A/en unknown
- 2002-07-19 DE DE60232622T patent/DE60232622D1/en not_active Expired - Lifetime
- 2002-07-19 EP EP02354113A patent/EP1279450B1/en not_active Expired - Lifetime
- 2002-07-25 KR KR1020020043924A patent/KR100866294B1/en not_active IP Right Cessation
- 2002-07-25 JP JP2002217045A patent/JP4118626B2/en not_active Expired - Fee Related
- 2002-07-26 CN CNB021270422A patent/CN1197674C/en not_active Expired - Fee Related
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| CN101844229A (en) * | 2010-03-24 | 2010-09-29 | 峨嵋半导体材料研究所 | Preparation method and production equipment of high-purity antimony particles |
| CN105170022A (en) * | 2014-06-16 | 2015-12-23 | 新特能源股份有限公司 | Granulation apparatus, preparation method for preparing catalyst for silicon tetrachloride catalytic hydrogenation reaction, and silicon tetrachloride catalytic hydrogenation reaction method |
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| WO2019024419A1 (en) * | 2017-08-04 | 2019-02-07 | 米亚索乐装备集成（福建）有限公司 | Atomization device and method for preparing metal alloy powder |
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| CN110090596A (en) * | 2018-01-30 | 2019-08-06 | 徐州市禾协肥业有限公司 | A kind of method and its fertiliser granulates of inclined-plane cooling granulation |
| CN110090596B (en) * | 2018-01-30 | 2022-06-21 | 徐州市禾协肥业有限公司 | Inclined surface cooling granulation method and fertilizer granules thereof |
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| CN116921231A (en) * | 2023-07-31 | 2023-10-24 | 苏州荣文西邻精密科技有限公司 | Sorting equipment |
| CN116921231B (en) * | 2023-07-31 | 2024-01-23 | 苏州荣文西邻精密科技有限公司 | Sorting equipment |
Also Published As
| Publication number | Publication date |
|---|---|
| EP1279450B1 (en) | 2009-06-17 |
| JP4118626B2 (en) | 2008-07-16 |
| KR100866294B1 (en) | 2008-10-31 |
| MY127347A (en) | 2006-11-30 |
| DE60232622D1 (en) | 2009-07-30 |
| JP2003155505A (en) | 2003-05-30 |
| ATE433815T1 (en) | 2009-07-15 |
| TW577780B (en) | 2004-03-01 |
| US6676890B2 (en) | 2004-01-13 |
| SG103876A1 (en) | 2004-05-26 |
| US20030020213A1 (en) | 2003-01-30 |
| CN1197674C (en) | 2005-04-20 |
| EP1279450A1 (en) | 2003-01-29 |
| KR20030010532A (en) | 2003-02-05 |
| CA2393862A1 (en) | 2003-01-26 |
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